CN106076336A - A kind of preparation method of magnetic ferric oxide nano piece - Google Patents

A kind of preparation method of magnetic ferric oxide nano piece Download PDF

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CN106076336A
CN106076336A CN201610409620.XA CN201610409620A CN106076336A CN 106076336 A CN106076336 A CN 106076336A CN 201610409620 A CN201610409620 A CN 201610409620A CN 106076336 A CN106076336 A CN 106076336A
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solution
ferric oxide
solid
oxide nano
nano piece
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黄文艳
赵文昌
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Changzhou University
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Changzhou University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8668Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/40Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/34Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
    • H01F1/342Oxides
    • H01F1/344Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/112Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1124Metal oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702Hydrocarbons
    • B01D2257/7027Aromatic hydrocarbons
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708Volatile organic compounds V.O.C.'s

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Power Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
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  • Compounds Of Iron (AREA)

Abstract

The present invention discloses the preparation method of a kind of magnetic ferric oxide nano piece.In turn include the following steps: take 500mL FeCl2Solution, it is placed in 70~80 DEG C of water-baths of constant temperature, in solution, is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH weak solution, keep pH value to be 12~13, reaction 2~3h, proceed in autoclave, in 1h, be warmed up to 150~180 DEG C, continue reaction 4~8h, naturally cool to room temperature, forming the precipitation with layer structure, precipitate and separate in this process, deionization is washed 2~3 times;The solid obtaining precipitation joins in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio is 1:10~1:50, stirring 4~5h, precipitate and separate, the solid obtaining is after being washed with deionized 2~3 times, calcine at a temperature of 400~450 DEG C, remove lactate therein, i.e. can get a kind of ferric oxide nano piece.This structure is conducive to absorption and catalysis pollutant, is conducive to separating simultaneously.

Description

A kind of preparation method of magnetic ferric oxide nano piece
Technical field
The present invention relates to the exploitation of novel environmental pollution control material, particularly relate to the preparation side of a kind of ferric oxide nano piece Method.
Background technology
VOCs treatment refers to that the organic exhaust gas producing in industrial processes carries out the place adsorbed, filter, purify Science and engineering is made.Usual VOCs treatment has the benzene homologues VOCs treatment such as formaldehyde VOCs treatment, benzene toluene dimethylbenzene etc. Deng.Organic exhaust gas be usually present inflammable and explosive, poisonous and harmful, water insoluble, be dissolved in the big spy of organic solvent, intractability Point.Commonly used when VOCs treatment is organic exhaust gas active-carbon adsorption treatment method, Production by Catalytic Combustion Process, catalysis oxidation Multiple principles such as method, acid-base neutralization method, plasma method.Catalysis oxidation is a kind of both economical effective method.But need through Ji is suitable for blanket catalyst.
Nano-sized iron oxide has good weatherability, light resistance, magnetic and has good absorption and shielding to ultraviolet Effect, is a kind of important inorganic material.Have important in fields such as catalysis, function ceramics, magnetic material and transparent pigments Application.Nano-sized iron oxide has huge specific surface area, and skin effect is notable, is also a kind of good catalyst.Use nanoparticle The activity of the catalyst that son is made, selectivity are all higher than typical catalyst, and life-span length easily operates.To make of nano-sized iron oxide The hollow beads becoming, floats on the wastewater surface containing organic matter.The degraded utilizing sunshine to carry out organic matter can be accelerated at waste water Reason process.Nano-sized iron oxide has been directly used as the catalyst of high molecular polymer oxidation, reduction and synthesis, butylphenol Catalyzed by Nano-ferric Oxide Agent can make the rate of cleavage of oil improve 1~5 times, using the burning velocity of its solid propellant made as combustion catalyst relatively Conventional propellant can improve 1~10 times, and this is highly beneficial to manufacture high-performance rocket and guided missile.Nano-sized iron oxide can also be catalyzed Decomposition water, makes clean energy resource.
Made magnetic nanometer composite material can effectively prevent nanometer by magnetic nanoparticle being dispersed in certain matrix Intergranular mutual reunion, efficiently controls its particle size.To lead additionally, magnetic-particle is embedded in immiscible medium Cause some unusual Physical and chemical characteristics.
Hydrotalcite-based compound (LDHs) is the compound piled up by interlayer anion and positively charged laminate.Neatly Stone chemical structure of general formula is: [M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+And M3+It is respectively positioned at main body laminate On divalence and trivalent metal cation, such as Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+Deng bivalent cation and Al3 +、Cr3+、Co3+、Fe3+All can form hydrotalcite Deng Tricationic;An–For interlayer anion, inorganic anion can be included, Organic anion, complex anion, same many and heteropolyanion;X is M3+/(M2++M3+) molar ratio, about 4:1 arrives 2:1;M is the number of intermediary water molecule.It is similar to that shepardite Mg (OH)2, octahedron is shared seamed edge and forms main body Laminate.The divalent metal M being positioned on laminate2+Can be golden by the close trivalent of ion half price in certain proportion Belong to cation M3+Same order elements so that laminate is positively charged, interlayer exist can exchange anion and laminate on positive electricity Lotus balances so that the overall structure of LDHs is electroneutral.The anion of interlayer can be exchanged, through a series of modifications, hydrotalcite Material can obtain many materials planting different properties.
Content of the invention
It is an object of the invention to, for overcoming the deficiency that iron oxide structure in prior art is single, provide a kind of ferric oxide nano The preparation method of piece.
The technical solution used in the present invention is in turn include the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2~3mol/L, take this solution of 500mL, Xiang Qi In be placed in 70~80 DEG C of water-baths of constant temperature, be simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH dilute molten Liquid, keeps pH value to be 12~13, reacts 2~3h, proceed in autoclave, be warmed up to 150~180 DEG C in 1h, continue reaction 4~ 8h, naturally cools to room temperature, forms the precipitation with layer structure, precipitate and separate in this process, and deionization is washed 2~3 times;
2) solid that precipitation obtains is joined in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio be 1:10~ 1:50, stir 4~5h, precipitate and separate, it is thus achieved that solid after being washed with deionized 2~3 times, the temperature of 400~450 DEG C The lower calcining of degree, removes lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
The invention have the advantage that the ferric iron that part ferrous ion is generated by hydrogen peroxide oxidation, divalent ion and generation Trivalent ion alkali in 70~80 DEG C of water-baths effect under, produce magnetic co-precipitation, form lamella hydrotalcite structure, then at piece Inter layer exchange enters lactate, removes lactate finally by high-temperature calcination, forms the lamellar structure relatively scattered.This structure has It is beneficial to absorption and catalysis pollutant.
Detailed description of the invention
3 embodiments of the offer present invention further below:
Embodiment 1
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, be placed in wherein In 80 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 4mL and a certain amount of NaOH weak solution, holding pH value is 13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 8h, naturally cool to room temperature, in this process Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times;The solid obtaining precipitation joins concentration In the sodium lactate solution of 4mol/L, solid-to-liquid ratio is 1:50, stir 5h, precipitate and separate, it is thus achieved that solid be washed with deionized 3 All over afterwards, calcine at a temperature of 450 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 97.2%, supernatant can be arranged Put.
Embodiment 2
By FeCl2It is dissolved in water, is configured to the solution that concentration is 2mol/L, take this solution of 500mL, be placed in wherein In 70 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2mL and a certain amount of NaOH weak solution, holding pH value is 12, react 2h, proceed in autoclave, in 1h, be warmed up to 150 DEG C, continue reaction 4h, naturally cool to room temperature, in this process Forming the precipitation with layer structure, precipitate and separate, deionization is washed 2 times;The solid obtaining precipitation joins concentration In the sodium lactate solution of 2mol/L, solid-to-liquid ratio is 1:10, stir 4h, precipitate and separate, it is thus achieved that solid be washed with deionized 2 All over afterwards, calcine at a temperature of 400 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 97.5%, supernatant can be arranged Put.
Embodiment 3
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, be placed in wherein In 80 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 3mL and a certain amount of NaOH weak solution, holding pH value is 13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 6h, naturally cool to room temperature, in this process Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times;The solid obtaining precipitation joins concentration In the sodium lactate solution of 4mol/L, solid-to-liquid ratio is 1:50, stir 5h, precipitate and separate, it is thus achieved that solid be washed with deionized 3 All over afterwards, calcine at a temperature of 450 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 94.3%, supernatant can be arranged Put.

Claims (1)

1. a preparation method for magnetic ferric oxide nano piece, is characterized in that in turn including the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2~3mol/L, take this solution of 500mL, be placed in wherein It in 70~80 DEG C of water-baths of constant temperature, is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH weak solution, protect Holding pH value is 12~13, reacts 2~3h, proceeds in autoclave, be warmed up to 150~180 DEG C in 1h, continues reaction 4~8h, from So being cooled to room temperature, forming the precipitation with layer structure, precipitate and separate in this process, deionization is washed 2~3 times;
2) joining the solid that precipitation obtains in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio is 1:10~1:50, Stirring 4~5h, precipitate and separate, it is thus achieved that solid after being washed with deionized 2~3 times, at a temperature of 400~450 DEG C Calcining, removes lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
CN201610409620.XA 2016-06-12 2016-06-12 A kind of preparation method of magnetic ferric oxide nano piece Pending CN106076336A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107899578A (en) * 2017-10-25 2018-04-13 浙江科技学院 A kind of heterogeneous class light fenton catalyst of rice-pudding shape micron ferric oxide and preparation method thereof
CN108186677A (en) * 2018-01-05 2018-06-22 中国科学院上海硅酸盐研究所 Degradable nano material that new free-radical efficiently generates and its preparation method and application

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107899578A (en) * 2017-10-25 2018-04-13 浙江科技学院 A kind of heterogeneous class light fenton catalyst of rice-pudding shape micron ferric oxide and preparation method thereof
CN107899578B (en) * 2017-10-25 2020-05-26 浙江科技学院 Zongzi-shaped micron-sized iron oxide heterogeneous photo-Fenton catalyst and preparation method thereof
CN108186677A (en) * 2018-01-05 2018-06-22 中国科学院上海硅酸盐研究所 Degradable nano material that new free-radical efficiently generates and its preparation method and application
CN108186677B (en) * 2018-01-05 2020-05-19 中国科学院上海硅酸盐研究所 Degradable nano material capable of efficiently generating free radicals and preparation method and application thereof

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Application publication date: 20161109